CN102507831A - Determination method of 1-deoxynojirimycin content in silkworm powder - Google Patents
Determination method of 1-deoxynojirimycin content in silkworm powder Download PDFInfo
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Abstract
A determination method of the 1-deoxynojirimycin content in silkworm powder relates to silkworm powder. The method comprises the following steps: weighing two 1-deoxynojirimycin control samples used as control liquid 1 and 2; sucking the control liquid 1 and 2, injecting the samples; weighing silkworm powder to be determined, adding petroleum ether, performing heating reflux and extraction in water bath, filtering, removing the filtrate, volatilizing the petroleum ether to dryness to obtain a product A; adding methanol in A, performing ultrasonic extraction, filtering, concentrating the filtrate, adding in a neutral alumina column, performing elution, collecting the eluted solution, evaporate to dryness, dissolving by methanol and obtaining a constant volume so as to used the solution as a test solution; performing HPLC analysis of the test solution, calculating the 1-deoxynojirimycin content in the silkworm powder to be determined by an external standard two-point method according to a peak area value. The method has the advantages of high precision, good repeatability and stability, qualified sample recovery rate, simplicity and practicality, and the like, can be popularized in general laboratories, and is applicable to the quality control of 1-deoxynojirimycin in silkworm powder products.
Description
Technical field
The present invention relates to a kind of silkworm powder, especially relate to a kind of method that adopts 1-DNJ content in the rp-hplc silkworm powder.
Background technology
The 1-DNJ is its hypoglycemic main active in the silkworm powder.1-DNJ and derivant thereof have efficiently pharmacological action widely, and diabetes and complication thereof, obesity, virus infections aspects such as (HIV) are had than notable therapeutic effect.How effectively to detect the quality of 1-DNJ product, creating a kind of method easy, that detect 1-DNJ content fast and efficiently becomes one of research focus gradually.The method of measuring 1-DNJ content mainly contains following four kinds:
First kind is the ion chromatography method, and Chen Zhiyi etc. utilize this method respectively 1-DNJ in yellow blood silkworm, the silkworm excrement to be carried out quantitative test.
Second kind is RPLC-fluorescence detection, and Ou Yangzhen etc., Jin etc. study this method respectively, and has measured the content of 1-DNJ in mulberry leaf and the silkworm powder.The result shows that the ion chromatography method has advantages such as sample preparation is simple, easy to operate, but separating effect and reliability are not ideal enough; RPLC-fluorescence detection, have highly sensitive, advantage such as the result is accurate, reliable, but the detecting device that requires costs an arm and a leg, seldom configuration receives than limitations aspect application popularization in the common laboratory.
The third is RPLC-uv detection method, though the used detecting device of this method is popularized in most laboratory, its sample needs pre-column derivatization, and derivatization process is complicated, and condition is difficult to be held.
The 4th kind, measure 1-DNJ in the silkworm body with EISD, this kind detecting device does not have UV-detector and fluorescence detector sensitivity.Therefore; Explore and a kind ofly just can measure the content of 1-DNJ in the complex mixture in common lab; And the sample preparation simpler method is the work that realistic meaning is quite arranged; Both can be provided at the analysis that common lab is carried out the 1-DNJ, and also be convenient to enterprise and carry out the 1-DNJ quality testing in the silkworm medicinal product production run.For this reason, explore the method for stablizing, detecting the 1-DNJ content in the silkworm sample accurately, the concrete technical parameter of research RP-HPLC-UV method obtains stable accurately mensuration result, has important practical significance.
Adopt the terminal absorption process of ultraviolet to detect 1-DNJ content in the silkworm powder, at home and abroad do not appear in the newspapers as yet at present.
Chinese patent CNl883513 discloses the separation method of active blood sugar-lowering substances in a kind of silkworm powder.Its separating step is at first with silkworm powder and the lixiviate damping fluid ratio mixing in 1: 1, puts lixiviate under 4～8 ℃ of environment, filtration, separation, carries out the extraction of the hypoglycemic effective constituent of silkworm powder; With ion-exchange chromatography on the leaching liquor of silkworm powder, carry out cation exchange column chromatography then, and adjustment pH value; Again wash-out, sample collection, concentrate and drying.This invention has kept the original active substance in the silkworm body, and blood-sugar decreasing active is single; Quantum of output is high, and pick-up rate is 2.7%.
Summary of the invention
The object of the present invention is to provide a kind ofly have not only that precision is higher, reappearance and stability better, advantage such as average recovery meets the requirements, method is simple and practical; And can popularize, and can be used for 1-DNJ Determination on content method in the silkworm powder of the quality control of 1-DNJ in the silkworm powder goods in common laboratory etc.
The present invention includes following steps:
1) claims to decide each two parts of 1-DNJ reference substances, as reference substance liquid 1 and reference substance liquid 2;
2) draw reference substance liquid 1 and reference substance liquid 2, sample introduction;
3) take by weighing silkworm powder to be measured, add sherwood oil, heating and refluxing extraction in water-bath is filtered, and discards filtrating, volatilizes sherwood oil, gets product A;
4) in product A, add methyl alcohol, ultrasonic Extraction is filtered, and will filtrate concentrates, and places the neutral alumina post again, and wash-out is collected elute soln, and evaporate to dryness is again with dissolve with methanol and constant volume, as need testing solution;
5) need testing solution of step 4) gained is carried out HPLC and analyzes, according to peak area value, with external standard two-point method calculation procedure 3) 1-DNJ content in the used silkworm powder to be measured.
In step 1), the concentration of said reference substance liquid 1 can be 0.82mg/mL, and the concentration of reference substance liquid 2 can be 0.74mg/mL.
In step 2) in, said absorption reference substance liquid 1 and reference substance liquid 2 can be each 10 μ l.
In step 3), said silkworm powder to be measured can be 0.5～2g for every part, and the amount that adds sherwood oil can be 15～60mL; Said in water-bath the time of heating and refluxing extraction can be 0.5～2h.
In step 4), the amount that in product A, adds methyl alcohol can be 15～60mL; The time of said ultrasonic Extraction can be 0.5～2h; Said will filtrating concentrates, and can be concentrated into 1～10mL; Said wash-out can adopt 0.02mol/L HCl wash-out and regulate flow velocity to 20～60 droplet/min.
In step 5), said HPLC analyzes and can adopt the high performance liquid chromatograph that includes UV-detector to detect, and detects wavelength and can be 190～400nm, and the stationary phase of used high performance liquid chromatography is a reverse-phase chromatographic column, and column temperature can be 20～50 ℃; Said moving phase can be the mixed liquor of water and acetonitrile; Wherein the ratio of organic phase can be 20%～90%, is 100% in the moving phase quality, and water shared mass percent in moving phase can be 10%～80%; Preferred 20%～70%, be preferably 30%～60%.
Key point of the present invention is, under above-mentioned moving phase and wavelength condition, can measure silkworm powder and preparation thereof very exactly in the content of 1-DNJ.
Outstanding advantage of the present invention and technique effect are mainly reflected in following several respects:
1) high performance liquid chromatography of being set up has characteristics such as simple to operate, that accuracy is high, selectivity is strong;
2) present, the general assay method of 1-DNJ all needs pre-column derivatization or directly detects with EISD, and the used detection method of the present invention need not the pre-column derivatization operation, has efficient, quick, oligosaprobic advantage;
3) the present invention adopts the terminal absorption process of ultraviolet to detect 1-DNJ content in the silkworm powder, at present, does not at home and abroad appear in the newspapers as yet; Method is easy, practical; Can popularize in common laboratory, it is stable to measure reliable results, can be used for the quality control of 1-DNJ in the silkworm powder goods.
Description of drawings
Fig. 1 is the typical curve of 1-DNJ.In Fig. 1, horizontal ordinate is 1-DNJ concentration (μ g), and ordinate is a peak area.
Embodiment
Following examples will combine accompanying drawing that the present invention is further described.
1-DNJ content assaying method is following in the silkworm powder:
Claim fixed two parts of 1-DNJ reference substances that quality is 8.20mg and 7.40mg, being mixed with concentration respectively is 0.82mg/mL, 0.74mg/mL, as reference substance liquid 1 and reference substance liquid 2.
Draw reference substance liquid 1 and reference substance liquid 2 each 10 μ l, each sample introduction once.
Taking by weighing lot number respectively is 200801,200802 and 200,803 3 batches of silkworm powders, and each 3 parts, every part of 1g adds sherwood oil 30mL respectively, and heating and refluxing extraction 1h in water-bath filters, and discards filtrating, volatilizes solvent.Add methyl alcohol 30mL, ultrasonic Extraction 1h filters, and filtrating is concentrated into 3mL; Be placed on the neutral alumina post,, regulate flow velocity to 40 droplet/min, collect elute soln 100mL with 0.02mol/L HCl wash-out; Evaporate to dryness, dissolve with methanol also is settled to 10mL, as need testing solution.
Carry out HPLC and analyze, according to peak area value, with 1-DNJ content in the external standard two-point method calculation sample.Through calculating, 1-DNJ content is 0.5957% in the silkworm powder sample, and the result is as shown in table 1 for different batches silkworm powder 1-DNJ assay.
Table 1 different batches silkworm powder 1-DNJ assay
Detect the selection of wavelength
1-DNJ molecule lacks conjugated double bond structures, uv absorption a little less than, need derive when it is carried out ultraviolet detection, or adopt terminal the absorption.This experiment is before analyzing with high performance liquid chromatograph; Get test sample and reference substance solution respectively; Carry out ultraviolet-visible spectrum scanning at 190-400nm, the wild buttocks of N-methyl isophthalic acid-deoxidation as a result is mould to have end to absorb at the 192nm place, and the final 203nm of selection of experiment detects wavelength.
The selection of moving phase
When adopting terminal absorbing wavelength to detect; Chromatogram flow phase adopts the low acetonitrile (the ultraviolet cut-on wavelength is 190nm) of cutoff wavelength; Can reduce the terminal interference that absorbs of ultraviolet, so this experiment optimizes to the proportioning of acetonitrile and water, respectively with acetonitrile-water (85: 15), (78: 22) and (75: 25) as moving phase; The result finds that the main peak retention time is 23.618min when acetonitrile-water (85: 15); During acetonitrile-water (78: 22), the main peak retention time is 11.487min; During acetonitrile-water (75: 25), the main peak retention time is 9.325min, but the major component separation separates relatively poor with impurity.So finally select acetonitrile-water (78: 22) as moving phase.
The selection of chromatographic column
At first adopting with the octadecyl silane is the chromatographic column of stationary phase, the result find the 1-DNJ on this chromatographic column without reserve.Analyzing reason, is that polarity is very big, C because 1-DNJ structure is with sugared closely similar in the silkworm powder
18Post can not effectively keep, so select amino chromatographic column (Hypersil NH for use
2Chromatographic column), chromatographic condition is optimized, can be with impurity and 1-DNJ well separated.
Typical curve is drawn
Precision takes by weighing 1-DNJ reference substance in right amount in volumetric flask, adds methyl alcohol to scale, shakes up to such an extent that concentration is the 1-DNJ titer of 1mg/mL.
Draw 2mL, 4mL, 6mL, 8mL, 10mL titer (concentration is 1mg/mL) successively, put in the 10mL measuring bottle, be diluted to scale with methyl alcohol, mixing.Draw 10 μ l respectively, measure respectively by above-mentioned chromatographic condition, the relational result of silkworm powder 1-DNJ concentration and peak area is as shown in table 2.
The relation of table 2 silkworm powder 1-DNJ concentration and peak area
With the chromatographic peak area is ordinate, and 1-DNJ concentration is horizontal ordinate, and the drawing standard curve is as shown in Figure 1; With 1-DNJ concentration peak area is carried out regretional analysis, draw its regression equation and be: Y=261320x, correlation coefficient r=0.9996; The result shows; 1-DNJ concentration is in 2～10 μ g scopes, and its concentration presents the good linear relation with corresponding peak area, and it is reliable in this scope, calculating its content according to peak area.
The reappearance test
Take by weighing the about 10g of neutral alumina (100 order) powder, 20mL is moistening with the 0.02mol/LHCL eluent, and fully stirring the disposable specification of packing in back is the glass chromatography column of 1.5cm * 20cm; Constantly rap tube wall, make evenly closely, with eluent 50mL drip washing; The envelope post, for use.
Take by weighing silkworm powder 1g to be measured, add sherwood oil 30mL, heating and refluxing extraction 1h in water-bath filters, and discards filtrating, volatilizes solvent.The accurate methyl alcohol 30mL that adds, ultrasonic Extraction 1h filters, and filtrating is concentrated into 3mL; Be placed on the neutral alumina post,, regulate flow velocity to 40 droplet/min, collect elute soln 100mL with 0.02mol/L HCl wash-out; Evaporate to dryness, dissolve with methanol also is settled to 10mL, as need testing solution.
Get 6 parts of silkworm powders, every part of about 1g presses the operation of sample size assay method behind the precision weighing, carry out HPLC and analyze, according to peak area value, with 1-DNJ content in the external standard two-point method calculation sample.The average content of measuring the 1-DNJ for 6 times is 0.5932%, its RSD=2.11%.This result shows that reappearance of the present invention is good, and reproducible test results is seen table 3.
Table 3 reproducible test results
Stability test
The same concentration test sample liquid 10 μ l of accurate absorption; Every separated 12h sample introduction once advances 5 times altogether, the record peak area value; The result measures the RSD=1.47% (referring to table 4) of 1-DNJ content in 72h, show that the 1-DNJ in the test sample is stable in 72h.
Table 4 stability test result
The average recovery test
Get 6 parts of the silkworm powders of known content, every part of about 0.5g adds reference substance 2.0012mg respectively and operates by the 2.2.2 method behind the precision weighing; Carry out HPLC and analyze, measure 1-DNJ content, calculate average recovery; The result sees that table 5 average recovery rate is 97.21%, RSD=2.55%.This result shows that this assay method meets the requirement of average recovery.
Table 5 silkworm powder 1-DNJ recovery test
Claims (10)
1. 1-DNJ Determination on content method in the silkworm powder is characterized in that may further comprise the steps:
1) claims to decide each two parts of 1-DNJ reference substances, as reference substance liquid 1 and reference substance liquid 2;
2) draw reference substance liquid 1 and reference substance liquid 2, sample introduction;
3) take by weighing silkworm powder to be measured, add sherwood oil, heating and refluxing extraction in water-bath is filtered, and discards filtrating, volatilizes sherwood oil, gets product A;
4) in product A, add methyl alcohol, ultrasonic Extraction is filtered, and will filtrate concentrates, and places the neutral alumina post again, and wash-out is collected elute soln, and evaporate to dryness is again with dissolve with methanol and constant volume, as need testing solution;
5) need testing solution of step 4) gained is carried out HPLC and analyzes, according to peak area value, with external standard two-point method calculation procedure 3) 1-DNJ content in the used silkworm powder to be measured.
2. 1-DNJ Determination on content method is characterized in that in step 1) in the silkworm powder as claimed in claim 1, and the concentration of said reference substance liquid 1 is 0.82mg/mL, and the concentration of reference substance liquid 2 is 0.74mg/mL.
3. 1-DNJ Determination on content method is characterized in that in step 2 in the silkworm powder as claimed in claim 1) in, said absorption reference substance liquid 1 is 10 μ l, said reference substance liquid 2 is 10 μ l.
4. 1-DNJ Determination on content method is characterized in that in step 3) in the silkworm powder as claimed in claim 1, and said silkworm powder to be measured is 0.5～2g for every part, and the amount that adds sherwood oil is 15～60mL.
5. 1-DNJ Determination on content method is characterized in that in step 3) in the silkworm powder as claimed in claim 1, said in water-bath the time of heating and refluxing extraction be 0.5～2h.
6. 1-DNJ Determination on content method is characterized in that in step 4) in the silkworm powder as claimed in claim 1, and the amount that in product A, adds methyl alcohol is 15～60mL.
7. 1-DNJ Determination on content method is characterized in that in step 4) in the silkworm powder as claimed in claim 1, and the time of said ultrasonic Extraction is 0.5～2h; Said will filtrating concentrates, and is to be concentrated into 1～10mL; Said wash-out adopts 0.02mol/L HCl wash-out and regulates flow velocity to 20～60 droplet/min.
8. 1-DNJ Determination on content method in the silkworm powder as claimed in claim 1; It is characterized in that in step 5); It is to adopt the high performance liquid chromatograph that includes UV-detector to detect that said HPLC analyzes; The detection wavelength is 190～400nm, and the stationary phase of used high performance liquid chromatography is a reverse-phase chromatographic column, and column temperature is 20～50 ℃; Said moving phase is the mixed liquor of water and acetonitrile, and wherein the ratio of organic phase is 20%～90%, is 100% in the moving phase quality, and water shared mass percent in moving phase is 10%～80%.
9. 1-DNJ Determination on content method in the silkworm powder as claimed in claim 8 is characterized in that said water shared mass percent in moving phase is 20%～70%.
10. 1-DNJ Determination on content method in the silkworm powder as claimed in claim 9 is characterized in that said water shared mass percent in moving phase is 30%～60%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103091421A (en) * | 2013-01-16 | 2013-05-08 | 浙江大学 | Determination method of content of 1-deoxynojirimycin in silkworm larvae |
| CN104007205A (en) * | 2014-06-13 | 2014-08-27 | 漳州片仔癀药业股份有限公司 | Method for detecting pharmaceutical preparation for treating xiaoke disease |
| CN104007206A (en) * | 2014-06-13 | 2014-08-27 | 漳州片仔癀药业股份有限公司 | Method for detecting silkworm excrement medicinal materials |
| CN110632187A (en) * | 2018-11-23 | 2019-12-31 | 西北农林科技大学 | Method for determining D-buckwheat alkali in buckwheat by using pre-column derivatization high performance liquid chromatography-fluorescence detector |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091421A (en) * | 2013-01-16 | 2013-05-08 | 浙江大学 | Determination method of content of 1-deoxynojirimycin in silkworm larvae |
| CN104007205A (en) * | 2014-06-13 | 2014-08-27 | 漳州片仔癀药业股份有限公司 | Method for detecting pharmaceutical preparation for treating xiaoke disease |
| CN104007206A (en) * | 2014-06-13 | 2014-08-27 | 漳州片仔癀药业股份有限公司 | Method for detecting silkworm excrement medicinal materials |
| CN110632187A (en) * | 2018-11-23 | 2019-12-31 | 西北农林科技大学 | Method for determining D-buckwheat alkali in buckwheat by using pre-column derivatization high performance liquid chromatography-fluorescence detector |
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